WO2021149839A1 - Soufre modifié et sa méthode de préparation - Google Patents

Soufre modifié et sa méthode de préparation Download PDF

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Publication number
WO2021149839A1
WO2021149839A1 PCT/KR2020/000935 KR2020000935W WO2021149839A1 WO 2021149839 A1 WO2021149839 A1 WO 2021149839A1 KR 2020000935 W KR2020000935 W KR 2020000935W WO 2021149839 A1 WO2021149839 A1 WO 2021149839A1
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WO
WIPO (PCT)
Prior art keywords
sulfur
modified sulfur
acid
modifier
temperature
Prior art date
Application number
PCT/KR2020/000935
Other languages
English (en)
Korean (ko)
Inventor
안필호
Original Assignee
안필호
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 안필호 filed Critical 안필호
Priority to US16/963,146 priority Critical patent/US11975966B2/en
Priority to KR1020227021428A priority patent/KR20220119622A/ko
Priority to GB2011636.4A priority patent/GB2599888A/en
Priority to AU2020213268A priority patent/AU2020213268A1/en
Priority to EP20915581.1A priority patent/EP4095090A1/fr
Priority to CN202080097705.3A priority patent/CN115210178A/zh
Priority to KR1020207021380A priority patent/KR102415829B1/ko
Priority to PCT/KR2020/000935 priority patent/WO2021149839A1/fr
Priority to CA3089617A priority patent/CA3089617A1/fr
Publication of WO2021149839A1 publication Critical patent/WO2021149839A1/fr
Priority to ZA2022/08405A priority patent/ZA202208405B/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/02Preparation of sulfur; Purification
    • C01B17/0221Melting
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/16Sulfur-containing compounds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/04Portland cements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/36Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing sulfur, sulfides or selenium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/02Preparation of sulfur; Purification
    • C01B17/0243Other after-treatment of sulfur
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/22Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

Definitions

  • DCPD dicyclopentadiene
  • an exemplary embodiment of the present specification includes a first step of mixing sulfur and an unsaturated fatty acid-based modifier; a second step of putting the mixture into a reactor and melting it by heating it to a temperature of 100°C or higher and 130°C or lower; a third step of raising the temperature of the melt to a temperature of 130 °C or higher and 200 °C or lower; and a fourth step of terminating the reaction when the viscosity of the melt becomes 6,000 cP or more and 25,000 cp or less at 160 °C.
  • Example 3 is a diagram illustrating the measurement of water absorption in Example 4-1 and Comparative Example 4-1.
  • the modified sulfur has spinnability.
  • spinnability can be expressed as stringiness, thread pullability, etc., and whether or not it has spinnability is an experiment in which a glass stick is put in and then removed from a mixture or reactant in a solution state in the manufacturing process of modified sulfur.
  • the mixture or reactant can be defined as having spinnability.
  • 5 is a view showing a microstructure photograph (x750) of modified sulfur according to an exemplary embodiment of the present specification. 5, it can be confirmed that the modified sulfur according to an exemplary embodiment of the present specification includes a microstructure, and specifically, it can be confirmed that the modified sulfur according to an exemplary embodiment of the present specification includes a fibrous tissue.
  • the content of the dicyclopentadiene-based modifier is 0.01 parts by weight or more and 5 parts by weight or less based on 100 parts by weight of sulfur.
  • the content of the second modifier is 10 parts by weight or more, 300 parts by weight based on 100 parts by weight of sulfur. is below.
  • the sulfonate-based anionic surfactant includes dodecyl benzene sulfonate including ABS (alkyl benene sulfonate) and LAS (linear alkyl benzene sulfonate); hydrotropes, short tail alkyl-benzene sulfonate; alpha-olefin sulfonates; lignosulfonate; A sulfo-carboxylic compound including sodium lauryl sulfoacetate may be included, but the present invention is not limited thereto.
  • the other anionic surfactants include organo phosphored surfactants; It may include, but is not limited to, an alkyl amino acid including lauryl sarcosinate, sarcosine, and the like.
  • Examples of the alcohol-based solvent include methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, isobutanol, hexanol, isopropyl alcohol, ethoxyethanol, ethyl lactate, octanol isopropyl alcohol, Ethylene glycol monomethyl ether, benzyl alcohol, 4-hydroxy-3-methoxy benzaldehyde, isodeconol, butylcarbitol, terpineol, alpha terpineol, beta-terpineol, cineol and It may be any one selected from the group consisting of combinations thereof, but is not limited thereto.
  • the fourth step of terminating the reaction may be performed according to the use by measuring the state and viscosity of the melt three or more times per hour.
  • the prepared modified sulfur may be for room temperature asphalt, modified sulfur polymer concrete, and has a viscosity of 6,000 cP or more and 25,000 cP at 160 ° C.
  • the prepared modified sulfur may be used for a waterproof paint or a rust preventive paint.
  • reaction termination time may be between the time point at which the reaction is radioactive and the time point at which the rubberization of the stage before carbonization is in progress
  • modified sulfur includes a microstructure shape of fibrous, honeycomb structure, and network structure, or radioactive properties. may be having
  • the method further includes the step of aging before the fourth step, wherein the aging step is performed at a temperature of 40° C. or higher for the melt.
  • the reaction termination time of the heated melt in the third step may be adjusted just before it has radioactivity, and the viscosity of the modified sulfur may be adjusted according to the intended use.
  • the characteristics of the modified sulfur may be adjusted by adjusting the input timing, type, and amount of the initiator according to the use of the modified sulfur.
  • the recycled industrial waste is, for example, a waste stone powder sludge obtained by precipitating stone powder generated when crushing aggregates with a sodium acrylate copolymer polymer coagulant, and is treated as waste and having difficulty in landfilling. Meaning, if it is industrial waste that can be used as the aggregate, it can be applied as the recycled industrial waste, and is not limited to waste stone powder sludge.
  • the concrete composition according to an exemplary embodiment of the present specification can be used in place of epoxy or urethane, is eco-friendly, and does not require overlapping construction of top coat, intermediate coat, and undercoat like the existing epoxy or urethane with one-time construction, so time and cost economical in terms of
  • modified sulfur crush 200 g of rubberized solid form of modified sulfur, add 10 g of diluent ethanol to give fluidity, and first mix 1000 g of aggregate (13 mm), 2 kg of sand and 150 g of MgO as a hardener at room temperature. After that, put it in a small aggregate mixer, pour the diluted modified sulfur and mix for 5 minutes, compact it 65 times with an asphalt specimen compactor, and after one day after demolding, put it in a hot water tank and immerse it in water at 60°C for 1 hour, then measure the stability value The silver 12286 flow value 21 was measured.
  • Example 2-3 it was confirmed that a good stability value and flow value were measured even when the content of the curing agent was reduced and mixed in the preparation of the specimen.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Lubricants (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

Abstract

La présente invention concerne un soufre modifié et sa méthode de préparation, le soufre modifié comprenant du soufre et un modificateur, le modificateur étant un modificateur à base d'acide gras insaturé.
PCT/KR2020/000935 2020-01-20 2020-01-20 Soufre modifié et sa méthode de préparation WO2021149839A1 (fr)

Priority Applications (10)

Application Number Priority Date Filing Date Title
US16/963,146 US11975966B2 (en) 2020-01-20 2020-01-20 Modified sulfur and production method thereof
KR1020227021428A KR20220119622A (ko) 2020-01-20 2020-01-20 개질 유황 및 이의 제조 방법
GB2011636.4A GB2599888A (en) 2020-01-20 2020-01-20 Modified sulfur and production method thereof
AU2020213268A AU2020213268A1 (en) 2020-01-20 2020-01-20 Modified sulfur and production method thereof
EP20915581.1A EP4095090A1 (fr) 2020-01-20 2020-01-20 Soufre modifié et sa méthode de préparation
CN202080097705.3A CN115210178A (zh) 2020-01-20 2020-01-20 改性硫及其生产方法
KR1020207021380A KR102415829B1 (ko) 2020-01-20 2020-01-20 개질 유황 및 이의 제조 방법
PCT/KR2020/000935 WO2021149839A1 (fr) 2020-01-20 2020-01-20 Soufre modifié et sa méthode de préparation
CA3089617A CA3089617A1 (fr) 2020-01-20 2020-01-20 Soufre modifie et sa methode de production
ZA2022/08405A ZA202208405B (en) 2020-01-20 2022-07-27 Modified sulfur and preparation method therefor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/KR2020/000935 WO2021149839A1 (fr) 2020-01-20 2020-01-20 Soufre modifié et sa méthode de préparation

Publications (1)

Publication Number Publication Date
WO2021149839A1 true WO2021149839A1 (fr) 2021-07-29

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/KR2020/000935 WO2021149839A1 (fr) 2020-01-20 2020-01-20 Soufre modifié et sa méthode de préparation

Country Status (9)

Country Link
US (1) US11975966B2 (fr)
EP (1) EP4095090A1 (fr)
KR (2) KR20220119622A (fr)
CN (1) CN115210178A (fr)
AU (1) AU2020213268A1 (fr)
CA (1) CA3089617A1 (fr)
GB (1) GB2599888A (fr)
WO (1) WO2021149839A1 (fr)
ZA (1) ZA202208405B (fr)

Families Citing this family (3)

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Publication number Priority date Publication date Assignee Title
CN112375253A (zh) * 2020-10-26 2021-02-19 贵州大学 橡胶用改性硫磺与白炭黑共混物的制备方法
CN113880056A (zh) * 2021-10-29 2022-01-04 雅邦绿色过程与新材料研究院南京有限公司 一种利用化学硫磺制备亲水性硫磺微球的方法
KR102449416B1 (ko) * 2022-04-14 2022-09-30 주식회사 엔투하이텍 내구성 및 항균성이 우수한 합성목재 및 이의 제조방법

Citations (3)

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KR20110037127A (ko) * 2009-10-05 2011-04-13 주식회사 하슬라 아미노산 개질유황 결합재 및 이의 제조방법
KR20140000160A (ko) 2012-06-22 2014-01-02 한국과학기술연구원 개질유황, 이의 제조방법, 및 이의 제조장치
WO2015112490A1 (fr) * 2014-01-21 2015-07-30 Agrium Advanced Technologies Soufre résistant aux chocs

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NL136779C (fr) * 1963-10-28
JP5286617B2 (ja) * 2008-10-15 2013-09-11 ハンミ イーアンドシー カンパニー リミテッド 改質硫黄結合材およびその製造方法と、これを含有する水硬性改質硫黄資材組成物およびその製造方法または可燃性改質硫黄資材組成物およびその製造方法
KR101308097B1 (ko) * 2009-09-22 2013-09-12 김종우 저융점 개질유황 결합재 및 이의 제조방법
KR20120096385A (ko) * 2011-02-22 2012-08-30 한미이엔씨 주식회사 개질 유황 결합재 및 그 제조 방법과, 이를 함유하는 수경성 개질 유황 자재 조성물 및 그 제조 방법 또는 가연성 개질 유황 자재 조성물 및 그 제조 방법
KR20120081957A (ko) * 2012-05-04 2012-07-20 한국과학기술연구원 상온에서 액상 형태를 유지하여 혼합 작업이 가능한 개질 유황 결합재 및 그 제조방법과, 이를 함유하는 수경성 개질유황자재 조성물 및 그 제조방법

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KR20140000160A (ko) 2012-06-22 2014-01-02 한국과학기술연구원 개질유황, 이의 제조방법, 및 이의 제조장치
WO2015112490A1 (fr) * 2014-01-21 2015-07-30 Agrium Advanced Technologies Soufre résistant aux chocs

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Also Published As

Publication number Publication date
GB2599888A (en) 2022-04-20
KR20220119622A (ko) 2022-08-30
KR102415829B1 (ko) 2022-07-01
US11975966B2 (en) 2024-05-07
CN115210178A (zh) 2022-10-18
EP4095090A1 (fr) 2022-11-30
GB202011636D0 (en) 2020-09-09
AU2020213268A1 (en) 2021-08-05
ZA202208405B (en) 2024-02-28
KR20210095993A (ko) 2021-08-04
CA3089617A1 (fr) 2021-07-20
US20210221682A1 (en) 2021-07-22

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